Jurnal Full Paper

Teknologi
EMULSION LIQUID MEMBRANE FOR Article history
Received
HEAVY METALS REMOVAL: EMULSION 7 January 2020
Received in revised form
BREAKING STUDY 10 July 2020
Accepted
Adhi Kusumastutia*, Samsudin Anisa, A. L. Ahmadb, B. S. 15 July 2020
Ooib, M. M. H. Shah Buddinc Published online
27 August 2020
aFaculty of Engineering, Universitas Negeri Semarang,
Kampus UNNES Sekaran, 50229, Semarang, Indonesia *Corresponding author
bSchool of Chemical Engineering, Engineering Campus, adhi_kusumastuti@mail.unnes.ac.id
USM, 14300, Nibong Tebal, Penang, Malaysia
cFaculty of Chemical Engineering, Universiti Teknologi

MARA, Shah Alam, Selangor 40450, Malaysia

Graphical abstract Abstract

Emulsion liquid membrane (ELM) method has been widely applied in the
separation process as the alternative of liquid/liquid extraction. This study
compared the application of microwave, ultrasonic probe, and centrifuge in
breaking the used emulsion. Demulsification efficiency was investigated in term
of water content in the membrane phase solution before and after
demulsification. The results showed that the use of microwave to break the used
emulsion provided demulsification efficiency of 98.10%, while application of
ultrasonic probe was able to break emulsion at efficiency of 98.45%. In the
meantime, demulsification efficiency of almost 97% was achieved when
employing centrifuge at centrifugation speed of 3000 rpm. Considering the
energy consumption, it is recommended to apply microwave irradiation for
emulsion breaking. It could save energy up to 97% and 99% compared to that of
ultrasonic probe and centrifuge, respectively.

Keywords: Emulsion liquid membrane, heavy metals, removal, emulsion

breaking, demulsification

Abstrak
Kaedah membran cecair emulsi (ELM) telah digunakan secara meluas dalam
proses pemisahan sebagai alternatif kepada penyarian cecair-cecair. Kajian ini
membandingkan aplikasi gelombang mikro, kuar ultrasonik, dan emparan untuk
memecahkan emulsi yang telah digunakan. Kecekapan pengemulsian diselidiki
dari segi kandungan air dalam larutan fasa membran sebelum dan selepas
demulsifikasi. Keputusan menunjukkan bahawa penggunaan gelombang mikro
untuk memecahkan emulsi yang digunakan mencapai kecekapan demulsifikasi
98.10%, manakala penggunaan kuar ultrasonik telah memecahkan emulsi pada
kecekapan 98.45%. Sementara itu, kecekapan demulsifikasi hampir 97% dicapai
apabila menggunakan emparan pada kelajuan 3000 rpm. Kaedah gelombang
mikro adalah disyorkan untuk memecahkan emulsi disebabkan penggunaan
tenaga yang kurang. Penjimatan tenaga untuk demulsifikasi adalah sehingga
97% bagi kaedah kuar ultrasonik dan 99% bagi kaedah emparan.

Kata kunci: Membran cecair emulsi, logam berat, penyingkiran, pecah emulsi,
demulsifikasi

© 2020 Penerbit UTM Press. All rights reserved

82:5 (2020) 51–57 | www.jurnalteknologi.utm.my | eISSN 2180–3722 |DOI: https://doi.org/10.11113/jt.v82.14539|

52 Adhi Kusumastuti et al. / Jurnal Teknologi (Sciences & Engineering) 82:5 (2020) 51–57
1.0 INTRODUCTION
Emulsion liquid membrane (ELM) is an established
technology as a modification of liquid/liquid
extraction. ELM has been considered as one of the
most attractive type of liquid membrane and more
selective than polymer-based membranes [1].
Moreover, most molecules have higher diffusivity
through liquids than that of through polymer
membranes, leading to higher extraction efficiency
[2]. In ELM method, extraction and stripping
processes occur in a single step thus make the
method economically feasible. ELM involves the
mixing of double emulsions, either water in oil in
water or oil in water in oil. External phase contains
impurities to be extracted. Membrane phase
composed of organic solution act as a barrier of
external and internal phases. The solute is transferred
through the membrane phase towards internal
phase [3, 4].
ELM system involves three main processes, i.e.
emulsification, extraction, and demulsification as
illustrated in Figure 1. Emulsion could be produced
using blender [5, 6], homogenizer [7, 8], ultrasonic
probe [9, 10], and stirrer [11]. Those researches
characterised the produced emulsion in term of
emulsion diameter, membrane breakage, and
emulsion swelling. The emulsion performance was
also tested in the extractions of various impurities.
Figure 1 Emulsion liquid membrane process
The ELM method has been widely applied in the
separation process. Heavy metal removals using ELM
have been intensively studied by many researchers.
Cadmium recoveries under ELM system have been
investigated by Ahmad, et al. [12], Kumbasar [13],
and Mortaheb, et al. [14]. Chromium extractions
have been studied by some other researchers [15-
17]. Other researchers conducted experiments on
copper removal by ELM [10, 18, 19]. High
concentration of copper is mostly available in the
wastewater of many industries such as metallurgy,
steel, paper and pulp, fertiliser, and petroleum
refining [20]. Beyond the maximum allowable
concentration of 1.3 ppm, copper is considered as
hazardous pollutant. Copper accumulation in
animals and humans may cause several disorders of
gastroenteritis, diarrhoea, anorexia, dehydration, and
shock, while chronic copper poisoning contributes to
Alzheimer’s, Memkes and Wilson’s diseases [21].
The last process in ELM system is demulsification.
The used emulsion must be broken that the
entrapped solutes could be recovered for further
necessities. The liquid membrane and internal phase
solution could be reused in the following
emulsification process. Emulsion breaking occurs
through three steps, i.e. flocculation, coagulation
and coalescence. In the first step, flocculation of the
dispersed droplets of internal phase occurs, forming
some larger groups. Furthermore, the drops in groups
coalesce into a large group, leads to the decrease
of drops numbers. Finally, due to gravity effect, the
large internal drops sink in the interface of membrane
and internal phase, coagulate with the water phase,
and generate the emulsion breaking [22].
There are several methods of demulsification [23],
i.e. chemical demulsification [24, 25], gravity or
centrifugal settling [26], pH adjustment, filtration,
heating treatment, electrostatic demulsification [27,
28], and membrane technique [29]. Demulsification
process based on the gravity effect occurs in a
centrifuge. Centrifugation accelerates sedimentation
of an immiscible mixture. Moreover, in the mixtures of
solutions in similar densities, gravity separations might
take hours. The use of centrifuge could minimise the
separation time to be few minutes. Centripetal force
could separate greater and lesser density solutions
leading to emulsion breaking [26].
Heating has also been used in demulsification, but
it is energy-intensive. Emulsion breaking is achieved
by applying heat. It has been known that surfactant
induces the formation of micelle by interactions of
polar hydrophilic head and non-polar hydrophobic
tail groups in the mixture. The applied heat interrupts
the micelle interactions leading to micelles
breakdown and liquids separation. Euston, et al. [30]
investigated destabilization of oil in water emulsion
by heat induction. They found that large increase of
emulsion breakdown occurred at degree of
hydrolysis > 27%. Electric field methods have been
used to demulsify water-in-oil emulsions [22]. It
promotes an irreversible rupturing of the stabilizing
emulsions and the droplets coalesce if the external
field exceeds a certain critical value. However, it is
ineffective for the water-in-oil emulsion having high
water content or a swelling. It can produce a
‘‘sponge’’ phase which contains abundant internal
aqueous phase in the interface of oil and aqueous
phase, so that demulsification efficiency is seriously
affected. Another demulsification method is
microwave irradiation. This process has similar
mechanism with that of dielectric heating. Internal
heating occurs when emulsion exposed to
electromagnetic field of microwave resulting in
molecular rotation and ionic conduction. It is
therefore accelerated the emulsion separation
process. Chan and Chen [31] investigated the
performance of microwave in breaking water in oil
53 Adhi Kusumastuti et al. / Jurnal Teknologi (Sciences & Engineering) 82:5 (2020) 51–57
emulsion by microwave irradiation by testing the
effects of emulsion conditions and microwave
operating conditions on the demulsification rate and
the separation efficiency of W/O emulsion.
In spite of the available reports of emulsion
breaking processes through many methods, there is
limited articles reveals the comprehensive studies of
demulsification in ELM system. Whereas ELM
performance also determined by successful
demulsification process. This study compared the
application of microwave, ultrasonic probe, and
centrifuge in breaking the used emulsion.
Demulsification efficiency was investigated in term of
water content in the membrane phase solution
before and after demulsification.
2.0 METHODOLOGY
2.1 Materials
The aqueous copper solutions were prepared by
dissolving copper nitrate (Merck) in deionised water.
HCl (Merck) was added to the feed solution to adjust
the pH. Trioctylamine (Merck) and Span 80 (Merck)
were used as extractant and surfactant, respectively.
Low odour kerosene purchased from Sigma Aldrich
was used as diluent. Ammonia (Merck) was used as
internal phase solution.
2.2 Procedures
After the extraction process, the organic membrane
phase was recovered for its diluents. The
demulsification processes using physical treatment
process were applied. The water content in the
emulsion before demulsification and in the
membrane phase after demulsification was
measured. The demulsification efficiency (Br) was
calculated as:
Br =
θ0 −θ1
× 100%
θ0 x(1−θ1 )
Br refers to demulsification efficiency, θ0 is the
fraction of water content in the emulsion before
demulsification, and θ1 is the fraction of water
content in the membrane phase after
demulsification. Energy consumption (Ec) for emulsion
breaking was determined as:
Ec = Pin x t
where Pin is the power consumed (J/s) and t is the
demulsification time (s).
2.1.1 Microwave Demulsification
A beaker glass was used to collect used emulsion. It
was then placed in defined position in the
microwave (domestic microwave oven, Panasonic,
NN-SM330 M) thus every experiment got the same
heating irradiation. Experiments were done at
irradiation power of 50 W, 380 W, 540 W, and 700 W
for 8 s, 10 s, 12 s, and 15 s irradiation time. The
irradiated sample was settled down until 15 minutes
and then collected for water content analysis.
2.1.2 Ultrasound Demulsification
Used emulsion was placed in a beaker glass. The 22.5
kHz ultrasonic irradiation (ultrasonic USG-150)
equipped with a titanium horn (3 mm diameter) was
mounted at the top of the cylindrical glass cell. The
emulsion was treated for 2, 4, 8, and 10 minutes at a
frequency of 20 kHz in different intensities of about
20%, 60%, and 80%. Water content analysis was also
done to the demulsified samples.
2.1.3 Centrifuge Demulsification
Certain volume of the used emulsion was put in the
centrifuge bottle. The demulsifying method was
conducted in a centrifuge (Kubota 5220) that
accelerates the sedimentation at 2500-3500 rpm. The
centrifugation time was varied from 5 to 15 minutes
with interval of 5 minutes. After centrifugation
process, the organic sample on the top layer of the
solution is collected for water content analysis.
GC-MS analysis by using a Perkin Elmer GC Clarus
680 MS Clarus SQ 8T was also applied to identify the
organic membrane phase after demulsification. The
length of column is 30 m with 250 µm of diameter.
Maximum temperature of oven was set at about
300oC. Helium was used as carrier gas with 0.8 ml/min
of flow rate. The sample was filtered by using a filter
paper before injected into the GC at one μl.
3.0 RESULTS AND DISCUSSION
3.1 Microwave Demulsification
(1) The used emulsion needs to be broken so that
membrane component can be reused for further
emulsification process. After demulsification, the
clear upper layer was sampled; pure kerosene
indicated the success of demulsification process. The
water content was then tested and the efficiency
was calculated using Equation 1. Study of Henry [32]
found that microwave irradiation was effective in
reducing emulsion stability at relatively high water
separation efficiency. It was also revealed that at
(2)
equal irradiation exposure time and power, emulsion
with higher water content achieved better
demulsification efficiency. This is due to the nature
properties of water, in which energy absorption of
water is higher than that of oil. Figure 1 shows the
effects of both microwave irradiation and settling
time on demulsification efficiency. It is seen that
demulsification efficiency increase with the increase
of irradiation and settling time. Right after separation
at irradiation time of 8 s, almost no separation of
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water and oil phase occurred thus resulted in very
low demulsification efficiency. Significant increase of
demulsification efficiency was seen after prolonging
settling times. Increment of demulsification rate by
the increase of microwave irradiation time is affected
by dielectric heating properties that able to separate
water-in-oil emulsions. The highest demulsification
efficiency of 82.45% was achieved by applying
irradiation time of 15 s and settling time of 15 min.
100
75
Efficiency (%)
3.2 Ultrasound Demulsification
Among the important factors affecting emulsions
breaking is sound intensity. In which, energy level is
varied depend on the sound intensities given to
emulsions. Dehydration process of emulsions is only
determined by mechanical effects of ultrasound. It
was revealed that the increment of sound intensity
resulted in the lower emulsion water content [34].
They found that the lowest water content was
achieved at sound intensity of 0.66 W/cm2, further
increase in sound intensity actually increased water
content. This also applies in this study, where sound

intensity of 60% resulted in the best demulsification

efficiency, shown in Figure 3. This is due to higher
50
sound intensity triggered the reduction of water-oil
Irradiation Time 8 s interface tension leading to emulsion breaking.
25 Irradiation Time 10 s However, further increment of sound intensity to be
Irradiation Time 12 s 80% leading to the decrease of demulsification
Irradiation Time 15 s efficiency. This is because excessive sound intensity
0
0 3 6 9 12 15 caused re-emulsification phenomenon [34].
Settling Time (mins)
100
Figure 1 Demulsification efficiency (Microwave power 540
W; Irradiation time: 8, 10, 12, and 15 s; settling time: 0, 3, 5,
75
10, 12, 15 mins) Efficiency (%)

50
Figure 2 reveals that very small amount of Intensity 20%
aqueous phase can be separated with a 50 W 25 Intensity 60%
power output. Even with power output above 380 W,
a critical settling time greater than 5 min was Intensity 80%
0
necessary to give significant raise in demulsification
0 5 10 15
rate. Along with settling time, demulsification rate
Irradiation Time (mins)
increases with the increase of microwave power. The
increase of microwave irradiation power resulted in Figure 3 Demulsification efficiency (Intensity: 20%, 60%, and
higher separation efficiency as well as sample 80%; Irradiation time: 2, 4, 8, 10 min)
temperature. Improvement of microwave irradiation
power from 50 W to 380 W gave insignificant effect of
demulsification efficiency. Neither did further 3.3 Centrifuge Demulsification
improvement to 540 W. Mohammed and
Mohammed [33] found that this phenomenon was Demulsification under centrifuge force was
triggered by the increase of wavelength and investigated in terms of time and speed. To see the
penetration depth as the increase of microwave compounds, some of the samples were tested using
power. GC-MS. The demulsification results are presented in
Figure 4.
100
100

75 90
Efficiency (%)

Efficiency (%)

50 80
Power 50 watts
70
Power 380 watts 2000 rpm
25 2500 rpm
Power 540 watts 60 3000 rpm
Power 700 watts
0 3500 rpm
50
3 6 9 12 15 5 10 15
Settling Time (mins) Demulsification Time (mins)

Figure 2 Demulsification efficiency (Irradiation time: 15 s; Figure 4 Demulsification efficiency (centrifugation speed:
Microwave power 50, 380, 540, and 700 W) 2000, 2500, 3000, and 3500 rpm; centrifugation time: 5, 10,
and 15 min)
55 Adhi Kusumastuti et al. / Jurnal Teknologi (Sciences & Engineering) 82:5 (2020) 51–57

It is revealed in Figure 4 that due to the principles of

gravity separation, increasing centrifugation speed
could enhance demulsification efficiency. Each
phase is separated due to the density difference
between each phase. Higher centrifugation speed
as well as longer centrifugation time is able to
accelerate the separation process. The graph also
shows that at centrifugation speed of 2000 rpm,
efficiency was governed by time. At 5 min, efficiency
was only about 86%, it gradually increased to be 90%
at 10 min, and at the end of the process it
succeeded to reach 92%. On the contrary, at high
centrifugation speed of 3500 rpm, there was no Figure 7 Demulsification efficiency (Total ion chromatogram
significant increase in efficiency with the time of demulsification process at 3000 rpm)
extension. At 5, 10, and 15 min of demulsification
process, the efficiencies were about 96%. It is also
seen that at 15 min, demulsification efficiency
increased from 95% at 2000 rpm to be 97% at 3500
rpm.
GC-MS testing was done and intended to verify
the compounds in the organic membrane phase
after demulsification process, which consists of
kerosene as a diluent and TOA as a carrier. For this
reason, the membrane phase obtained from
centrifuge demulsification process was selected and
used as the sample. In general, there were about 20
major compounds of total ion chromatogram (TIC) Figure 8 Demulsification efficiency (Total ion chromatogram
detected qualitatively from the organic membrane of demulsification process at 3500 rpm)
phase sample. GC-MS result for each centrifugation
speed was revealed in Figures 5-8. The figures define
that in retention time of 5-15 min, kerosene The increase of centrifugation speed from 2000
compounds were exclusively detected. TOA was rpm to 3500 rpm enabled the system to demulsify
detected at around 21 min and after 25 min of and to recover almost all of kerosene and TOA. It was
retention time for centrifugation speeds above and indicated from total ion chromatogram report that
below 3000 rpm, respectively. demulsification process was able to recover about
99% and 98.7% of TOA and kerosene in organic
membrane phase for 3500 rpm and 3000 rpm,
respectively. Whereas at 2000 rpm, less than 90% of
kerosene and TOA was able to be recovered while
at 2500 rpm, more kerosene and TOA of about 97%
was recovered.

3.4 Demulsification and Energy Consumption

Assessment

Demulsification processes done by microwave,

Figure 5 Demulsification efficiency (Total ion chromatogram
of demulsification process at 2000 rpm)
Figure 6 Demulsification efficiency (Total ion chromatogram
of demulsification process at 2500 rpm)
ultrasound, and centrifuge have been completed.
Comparison of each process is described in Figure 9.
It is seen that demulsification efficiency was in the
order of ultrasound > microwave > centrifuge.
However, there was no significant difference of
demulsification efficiency of each mode. In term of
energy consumption, there was tremendous
difference of each demulsification tool. Microwave
provided the most energy efficient demulsification
process. In this case, microwave demulsification only
used 16.875 kJ of energy or about 117 times lower
than that of centrifuge. While ultrasound, required
energy of about 600 kJ, was higher than that used of
microwave. The highest energy of 1980 kJ was
applied in centrifuge demulsification. It is therefore,
56 Adhi Kusumastuti et al. / Jurnal Teknologi (Sciences & Engineering) 82:5 (2020) 51–57
microwave demulsification is
recommended process.
100
90
Efficiency (%)
80
70
60
50
MICROWAVE ULTRASOUND CENTRIFUGE
Figure 9 Comparison of demulsification efficiency and
energy consumption for each demulsification equipment
4.0 CONCLUSION
Laboratory experiment showed the application of
microwave, ultrasonic probe, and centrifuge for
emulsion breaking. All the demulsification tools were
successfully applied to break the used emulsion
based on their specific operation condition. In
general, demulsification efficiencies of above 97%
were obtained. It was found that the order of
demulsification efficiency was centrifuge <
microwave < ultrasound. Although ultrasound
provided the highest demulsification efficiency, it
consumed more energy. Among the demulsification
tools, microwave demulsification involved the lowest
energy consumption. The significant difference of
energy consumption was also supported by almost
the same demulsification efficiency. So that,
considering the economics of overall emulsion liquid
membrane process, microwave irradiation is highly
recommended for breaking the used emulsion. It
should be noted that the water in the sample
absorbs microwave energy, resulting in heating due
to polarization of water molecules, leading to the
acceleration of the demulsification process. In this
study, 15 seconds of irradiation time was enough to
break the emulsion at high efficiency.
Acknowledgement
Fundamental research grant from Ministry of
Research, Technology, and Higher Education of
Indonesia is gratefully acknowledged.
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